CN109207985A - A kind of preparation method of Mg alloy surface high-entropy alloy film layer - Google Patents
A kind of preparation method of Mg alloy surface high-entropy alloy film layer Download PDFInfo
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- CN109207985A CN109207985A CN201811032588.3A CN201811032588A CN109207985A CN 109207985 A CN109207985 A CN 109207985A CN 201811032588 A CN201811032588 A CN 201811032588A CN 109207985 A CN109207985 A CN 109207985A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
Abstract
The present invention relates to a kind of preparation methods of Mg alloy surface high-entropy alloy film layer; it is the case where being directed to soft magnesium alloy quality, poor corrosion resistance; previously prepared high-entropy alloy powder and steel ball are placed in sample jar; using the method for surface high-energy shot; high-entropy alloy powder is set to combine closely in AZ31 Mg alloy surface by big mechanically deform; to form one layer of high-entropy alloy layer with protective effect in AZ31 Mg alloy surface, the surface mechanical performance and and corrosion resisting property of magnesium alloy is greatly improved in this method.The corrosion rate of surface alloying layer is approximately the 1.5% of substrate, and wearability can be improved more than one times.This preparation method simple process, magnitude is accurately full and accurate, and anchoring strength of coating is good, dense structure, is the film layer Enhancement Method of very ideal magnesium alloy.
Description
Technical field
The present invention relates to a kind of preparation methods of AZ31 Mg alloy surface high-entropy alloy film layer, and belonging to non-ferrous metal improves surface
The technical field of mechanical performance, corrosion resisting property and technique preparation.
Background technique
Magnesium and magnesium alloy are a kind of non-ferrous alloys, have density small, and specific strength and specific stiffness are high, electromagnetic wave shielding
Well, it the advantages that easy to process, is used widely in auto industry, electronic product, aerospace field；But its chemical activity
Height, poor corrosion resistance, easily oxidation generates loose porous oxide film in wet air, these drawbacks have limited magnesium
Application of the alloy in more areas carries out surface treatment right and wrong to magnesium alloy to be widely applied magnesium alloy more
It is often necessary.
Currently, the surface treatment method of magnesium alloy is there are many form, as chemical conversion treatment method, anodized method,
Organic coating method, PVD method, plating, surface spray metal etc., although these surface modifying methods have certain work to magnesium alloy
With, but there is also technical deficiencies, and some complex process, equipment investment is big, at high cost, some coatings and matrix associativity
Difference, easy to fall off, some coated substance performances are insufficient, and enhancing, hardening, corrosion resistant purpose is not achieved, in short, most of be all difficult to
Realize heavy industrialization application.
Summary of the invention
The present invention is the technologies such as complex process in the process for treating surface for solve current magnesium alloy, coated substance performance deficiency
Problem provides a kind of preparation method of Mg alloy surface high-entropy alloy film layer.
The present invention is achieved by the following technical scheme: a kind of preparation method of Mg alloy surface high-entropy alloy film layer,
Using following raw material: AZ31 magnesium alloy plate, nickel powder, iron powder, copper powder, chromium powder, cobalt powder；
The following steps are included:
(1) selected chemical substance material
It is as follows to the chemical substance quality of materials Pureness control used:
AZ31 magnesium alloy plate: 99.8% or more solid state；
Nickel powder: 99.0% or more solid state；
Iron powder: 99.0% or more solid state；
Copper powder: 99.0% or more solid state；
Chromium powder: 99.0% or more solid state；
Cobalt powder: 99.0% or more solid state；
(2) AZ31 magnesium alloy plate is handled
AZ31 plate is cut into the sample of 10mm*10mm*6mm, solution treatment is carried out to AZ31 sample at 420 DEG C, when heat preservation
Between be 15h, carry out water quenching after soaking time, then board samples surface ground, polish, is cleaned；
(3) ball milling is at high-entropy alloy powder
By nickel powder, iron powder, copper powder, chromium powder, cobalt powder according to etc. atomic ratios mix, be subsequently placed in ball mill and carry out ball milling, ball milling
Pill-rolling material is GCr15 steel；The ratio between ball milling pill-rolling and dusty material volume are 10:1, and rotational speed of ball-mill is 290 ~ 310r/min, nothing
Water-ethanol is process control agent, Ball-milling Time 1800min；
(4) prepared by high-entropy alloy film layer
AZ31 magnesium alloy sample is fixed at the top of the jar of high-energy shot equipment, high-entropy alloy powder obtained is put into jar
The GCr15 steel ball that diameter is the quality such as 8 mm, 6mm and 4mm is put into togerther in high-energy shot tank, the shake of high-energy shot by bottom
Dynamic frequency is 20kHz, and the shot-peening time is 30min.
The present invention has apparent advance compared with prior art, is soft, poor corrosion resistance for magnesium alloy quality
Previously prepared high-entropy alloy powder and steel ball are placed in sample jar by feature, using the method for surface high-energy shot, are passed through
Big mechanically deform makes high-entropy alloy powder combine closely in AZ31 Mg alloy surface, to form one in AZ31 Mg alloy surface
Layer has the high-entropy alloy layer of protective effect, and the surface mechanical performance and corrosion resistance of magnesium alloy is greatly improved in this method
Energy.
The preparation method of high-entropy alloy mixing fine powders of the present invention can guarantee that the high-entropy alloy fine powder prepared is conducive to
Shot-peening；Parameter used by shot-blast process can ensure that high-entropy alloy (mixing fine powders) can become during shot-peening by plasticity
Shape and substrate are closely linked.The surface of magnesium alloy is finally greatly improved in the combination of each related process and parameter
Intensity, hardness and corrosion resistance.And the corrosion rate of surface alloying layer is approximately the 1.5% of substrate, and wearability can be improved one times
It is more.
The present invention uses high-entropy alloy powder for superficial film material using AZ31 magnesium alloy as matrix, through nickel, iron, copper,
Chromium, cobalt dust mixing, ball milling, shot blasting on surface form high-entropy alloy film layer, to increase substantially the mechanics of surface of magnesium alloy
Energy and and corrosion resistance.This method avoid the diffusion heat treatments traditionally carried out to obtain the alloy coat of said function
The deterioration of caused matrix structure variation and mechanical property.This preparation method simple process, magnitude is accurately full and accurate, and coating combines strong
It spends, dense structure, is the coating Enhancement Method of very ideal magnesium alloy, can realize that batch is raw in Mg alloy surface processing
Produce application.
Detailed description of the invention
Fig. 1 is AZ31 sample surfaces high-entropy alloy film layer preparation process schematic diagram.
Fig. 2 is the SEM Cross Section Morphology that surface prepares high-entropy alloy film layer sample.
Fig. 3 is the EDS line scanning result curve in Fig. 2 at solid white line.
Fig. 4 is the XRD diagram of high-entropy alloy powder and surface high-entropy alloy film layer.
Fig. 5 is that the liberation of hydrogen rate that AZ31 substrate and film layer sample are immersed in 5wt.% NaCl solution and soaking time are closed
System's figure.
Fig. 6 is the polarization curve of AZ31 substrate and high-entropy alloy film layer.
Fig. 7 is SEM surface topography after the wear test of high entropy alloy coating.
Fig. 8 is SEM surface topography after the wear test of AZ31 magnesium alloy substrates.
Specific embodiment
The preparation method of a kind of Mg alloy surface high-entropy alloy film layer of embodiment 1, using following raw material: AZ31 magnesium alloy
Plate, nickel powder, iron powder, copper powder, chromium powder, cobalt powder；
The following steps are included:
(1) selected chemical substance material
It is as follows to the chemical substance quality of materials Pureness control used:
AZ31 magnesium alloy plate: 99.8% or more solid state；
Nickel powder: 99.0% or more solid state；
Iron powder: 99.0% or more solid state；
Copper powder: 99.0% or more solid state；
Chromium powder: 99.0% or more solid state；
Cobalt powder: 99.0% or more solid state；
(2) AZ31 magnesium alloy plate is handled
AZ31 plate is cut into the sample of 10mm*10mm*6mm, solution treatment is carried out to AZ31 sample at 420 DEG C, when heat preservation
Between be 15h, carry out water quenching after soaking time, then board samples surface ground, polish, is cleaned.
(3) ball milling is at high-entropy alloy powder
By nickel powder, iron powder, copper powder, chromium powder, cobalt powder according to etc. atomic ratios mix, be subsequently placed in ball mill and carry out ball milling, ball milling
Grinding ball material is GCr15 steel；The ratio between ball milling abrading-ball and dusty material volume are 10:1, rotational speed of ball-mill 290r/min, anhydrous second
Alcohol is process control agent, Ball-milling Time 1800min；
(4) prepared by high-entropy alloy film layer
AZ31 magnesium alloy sample is fixed at the top of the jar of high-energy shot equipment, high-entropy alloy powder obtained is put into jar
The GCr15 steel ball that diameter is the quality such as 8mm, 6mm and 4mm is put into togerther in high-energy shot tank, the vibration of high-energy shot by bottom
Frequency is 20kHz, and the shot-peening time is 30min.
The preparation method of a kind of Mg alloy surface high-entropy alloy film layer of embodiment 2, using following raw material: AZ31 magnesium alloy
Plate, nickel powder, iron powder, copper powder, chromium powder, cobalt powder；
The following steps are included:
(1) selected chemical substance material
It is as follows to the chemical substance quality of materials Pureness control used:
AZ31 magnesium alloy plate: 99.8% or more solid state；
Nickel powder: 99.0% or more solid state；
Iron powder: 99.0% or more solid state；
Copper powder: 99.0% or more solid state；
Chromium powder: 99.0% or more solid state；
Cobalt powder: 99.0% or more solid state；
(2) AZ31 magnesium alloy plate is handled
AZ31 plate is cut into the sample of 10mm*10mm*6mm, solution treatment is carried out to AZ31 sample at 420 DEG C, when heat preservation
Between be 15h, carry out water quenching after soaking time, then board samples surface ground, polish, is cleaned.
(3) ball milling is at high-entropy alloy powder
By nickel powder, iron powder, copper powder, chromium powder, cobalt powder according to etc. atomic ratios mix, be subsequently placed in ball mill and carry out ball milling, ball milling
Grinding ball material is GCr15 steel；The ratio between ball milling abrading-ball and dusty material volume are 10:1, rotational speed of ball-mill 300r/min, anhydrous second
Alcohol is process control agent, Ball-milling Time 1800min；
(4) prepared by high-entropy alloy film layer
AZ31 magnesium alloy sample is fixed at the top of the jar of high-energy shot equipment, high-entropy alloy powder obtained is put into jar
The GCr15 steel ball that diameter is the quality such as 8mm, 6mm and 4mm is put into togerther in high-energy shot tank, the vibration of high-energy shot by bottom
Frequency is 20kHz, and the shot-peening time is 30min.
The preparation method of a kind of Mg alloy surface high-entropy alloy film layer of embodiment 3, using following raw material: AZ31 magnesium alloy
Plate, nickel powder, iron powder, copper powder, chromium powder, cobalt powder；
The following steps are included:
(1) selected chemical substance material
It is as follows to the chemical substance quality of materials Pureness control used:
AZ31 magnesium alloy plate: 99.8% or more solid state；
Nickel powder: 99.0% or more solid state；
Iron powder: 99.0% or more solid state；
Copper powder: 99.0% or more solid state；
Chromium powder: 99.0% or more solid state；
Cobalt powder: 99.0% or more solid state；
(2) AZ31 magnesium alloy plate is handled
AZ31 plate is cut into the sample of 10mm*10mm*6mm, solution treatment is carried out to AZ31 sample at 420 DEG C, when heat preservation
Between be 15h, carry out water quenching after soaking time, then board samples surface ground, polish, is cleaned.
(3) ball milling is at high-entropy alloy powder
By nickel powder, iron powder, copper powder, chromium powder, cobalt powder according to etc. atomic ratios mix, be subsequently placed in ball mill and carry out ball milling, ball milling
Grinding ball material is GCr15 steel；The ratio between ball milling abrading-ball and dusty material volume are 10:1, rotational speed of ball-mill 310r/min, anhydrous second
Alcohol is process control agent, Ball-milling Time 1800min；
(4) prepared by high-entropy alloy film layer
AZ31 magnesium alloy sample is fixed at the top of the jar of high-energy shot equipment, high-entropy alloy powder obtained is put into jar
The GCr15 steel ball that diameter is the quality such as 8mm, 6mm and 4mm is put into togerther in high-energy shot tank, the vibration of high-energy shot by bottom
Frequency is 20kHz, and the shot-peening time is 30min.
Further include the storage to product: the soft dustless paper wrapper of high entropy alloy coating sample to preparation is placed in moisture-proof
It in cabinet, is corroded with waterproof, moisture-proof, anti-oxidation, anti-acid-alkali salt, storage temperature is 20 DEG C ± 3 DEG C, relative temperature≤10%.
The present invention will be further described below with reference to the accompanying drawings:
It is AZ31 sample surfaces high-entropy alloy film layer film forming procedure schematic diagram shown in Fig. 1.High-entropy alloy powder is attached to high energy ball
AZ31 Mg alloy surface is hit simultaneously in pellet in ball surface, high while substrate surface generates plastic deformation under high energy effect
Entropy alloy powder is incorporated in Mg alloy surface also by mechanical force.With the extension of time, high-entropy alloy gradually covers
Magnesium alloy whole surface, and the high-entropy alloy powder of subsequent pellet surface attachment is bonded under high energy effect and has been formed
Film layer most surface, repeatedly, film layer gradually thickeies.
It is the microstructure sectional view of the high-entropy alloy film layer of magnesium alloy sample surfaces shown in Fig. 2.As seen from the figure:
AZ31 substrate surface forms the film layer greater than 10 microns, and film layer is tightly combined with substrate.
It is the line scanning spectra of high-entropy alloy layer shown in Fig. 3.EDS analyzes the visible nickel of result, iron, copper, five kinds of chromium, cobalt members
The ratio between atomicity of element essentially 1:1:1:1:1.
It is the XRD diffraction spectrogram of mixed-powder and surface formation high-entropy alloy film layer sample after ball milling, by scheming shown in Fig. 4
Known to: handling the mixed-powder before the film layer and shot-peening that AZ31 magnesium alloy substrates surface is formed by high-energy shot is all high entropy
Alloy.
Shown in Fig. 5, the liberation of hydrogen rate and soaking time being immersed in 5wt.% NaCl solution for substrate and coating sample are closed
System's figure.As it can be seen that AZ31 magnesium alloy substrates not only gradually corrode with the extension of soaking time, but also presents and ramp up
The trend of corrosion.However, coating sample is almost without corroding.
Shown in Fig. 6, there is high entropy alloy coating sample to test acquisition AZ31 magnesium alloy substrate and surface through dynamic potential scanning
Polarization curve in 3.5wt.%NaCl solution.From figure this it appears that due to coating protection so that sample from rotten
Erosion current potential shuffles 2.1V, and corrosion electric current density declines 3 orders of magnitude, belongs to typical anodic control protection.According to Ta Feier
Epitaxy is it can be calculated that the corrosion rate of coating sample is only the 1.5% of substrate sample.
Shown in Fig. 7, for SEM surface topography after the wear-resistant experiment of high entropy alloy coating., it is apparent that coating sample is presented
The feature of an apparent adhesion wear out.The width of polishing scratch is 0.7mm.
Shown in Fig. 8, for SEM surface topography after the wear-resistant experiment of substrate.It can be seen that: in AZ31 substrate, mainly with rule
, the polishing scratch that ditch dug with a plow is the same be characterized, without plasticity hangover shape trace, be the characteristics of belonging to abrasive wear in a word.Polishing scratch
Width is 1.1mm.Discovery is compared with the SEM pattern of high-entropy alloy film layer, the wear-resisting property of substrate is poor.
Claims (1)
1. a kind of preparation method of Mg alloy surface high-entropy alloy film layer, it is characterised in that: use following raw material: AZ31 magnesium alloy
Plate, nickel powder, iron powder, copper powder, chromium powder, cobalt powder；
The following steps are included:
(1) selected chemical substance material
It is as follows to the chemical substance quality of materials Pureness control used:
AZ31 magnesium alloy plate: 99.8% or more solid state；
Nickel powder: 99.0% or more solid state；
Iron powder: 99.0% or more solid state；
Copper powder: 99.0% or more solid state；
Chromium powder: 99.0% or more solid state；
Cobalt powder: 99.0% or more solid state；
(2) AZ31 magnesium alloy plate is handled
AZ31 plate is cut into the sample of 10mm*10mm*6mm, solution treatment is carried out to AZ31 sample at 420 DEG C, when heat preservation
Between be 15h, carry out water quenching after soaking time, then board samples surface ground, polish, is cleaned；
(3) ball milling is at high-entropy alloy powder
By nickel powder, iron powder, copper powder, chromium powder, cobalt powder according to etc. atomic ratios mix, be subsequently placed in ball mill and carry out ball milling, ball milling
Grinding ball material is GCr15 steel；The ratio between ball milling abrading-ball and dusty material volume are 10:1, and rotational speed of ball-mill is 290 ~ 310r/min, nothing
Water-ethanol is process control agent, Ball-milling Time 1800min；
(4) prepared by high-entropy alloy film layer
AZ31 magnesium alloy sample is fixed at the top of the jar of high-energy shot equipment, high-entropy alloy powder obtained is put into jar
The GCr15 steel ball that diameter is the quality such as 8mm, 6mm and 4mm is put into togerther in high-energy shot tank, the vibration of high-energy shot by bottom
Frequency is 20kHz, and the shot-peening time is 30min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079798A (en) * | 2019-05-08 | 2019-08-02 | 中北大学 | A method of in titanium alloy sheet surface laser cladding titanium-chromium-aluminum-silicon nickel high-entropy alloy |
| CN112593225A (en) * | 2020-11-26 | 2021-04-02 | 江苏珀然股份有限公司 | Process method for preparing high-hardness corrosion-resistant hub coating |
| CN112899664A (en) * | 2021-01-27 | 2021-06-04 | 太原科技大学 | Magnesium alloy surface zirconia-based film and preparation method thereof |
| CN113634764A (en) * | 2021-07-26 | 2021-11-12 | 太原理工大学 | Method for manufacturing stainless steel-based composite coating on surface of magnesium alloy through laser additive manufacturing |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079798A (en) * | 2019-05-08 | 2019-08-02 | 中北大学 | A method of in titanium alloy sheet surface laser cladding titanium-chromium-aluminum-silicon nickel high-entropy alloy |
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| CN112899664A (en) * | 2021-01-27 | 2021-06-04 | 太原科技大学 | Magnesium alloy surface zirconia-based film and preparation method thereof |
| CN112899664B (en) * | 2021-01-27 | 2022-08-02 | 太原科技大学 | Magnesium alloy surface zirconia-based film and preparation method thereof |
| CN113634764A (en) * | 2021-07-26 | 2021-11-12 | 太原理工大学 | Method for manufacturing stainless steel-based composite coating on surface of magnesium alloy through laser additive manufacturing |
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Application publication date: 20190115 |